CN103657698A - Preparation method for nitrogen doped graphene-niobium pentoxide intercalation composite catalyst with high oxygen reduction performance - Google Patents
Preparation method for nitrogen doped graphene-niobium pentoxide intercalation composite catalyst with high oxygen reduction performance Download PDFInfo
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Abstract
The invention relates to a preparation method for nitrogen doped graphene-niobium pentoxide intercalation composite catalyst with a high oxygen reduction performance. The method comprises the following steps: mixing niobium pentoxide and potassium carbonate at the molar ratio of (3:1)-(3:1.5), heating to 600-1000 DEG C, keeping for 1 hour, then heating up to 1050-1300 DEG C, keeping for 1-10 hours; washing by hot water; drying for 1-72 hours at the temperature of 100-500 DEG C; placing obtained products in a 10-68wt% nitric acid solution, stirring for 1-7days; repeating for 2-5 times; filtering and washing by distilled water, drying for 1-72 hours at the temperature of 30-80 DEG C; mixing the product with 4-vinyl pyridine at the mass ratio of (1:0.2)-(1:5), then dispersing in water; stirring for 1-7 days at the room temperature; filtering and washing by the distilled water, performing vacuum drying for 1-72 hours at the room temperature; heating to 700-900 DEG C under the argon atmosphere, keeping the temperature for 1-10 hours, cooling and obtaining the target catalyst. The catalyst has extremely excellent catalysis effect in the oxygen reduction reaction, and delivers better stability, higher methanol tolerance and comparative initial potential fall than a conventional representative Pt/C catalyst.
Description
Technical field
The invention belongs to the field of physical chemistry, materials chemistry, organic chemistry intersection, the preparation method who relates to a kind of intercalation composite material of efficient oxygen reduction catalyst, is specifically related to the preparation method that a kind of nitrogen of hyperoxia reducing property is mixed Graphene-niobium pentaoxide intercalation composite material.
Background technology
In recent years, due to quick consumption and the reserves minimizing of fossil fuel, regenerative resource and the correlation technique with environmental friendliness, low price, efficient feature have attracted increasing sight (Liang Y.; Li Y; Wang H.; Zhou J.; Wang J.; Regier T.; Dai H.
nature Mater. 2011,
10, 780-786.).Oxygen reduction reaction (Oxygen Reduction reaction, ORR) all has great significance to the application of a lot of regenerative resources, as metal-air battery, and water decomposition, (the Liang Y. such as fuel cell; Wang H.; Diao P.; Chang W.; Hong G.; Li Y.; Gong M.; Xie L.; Zhou J.; Wang J.; Regier T. Z.; Wei F.; Dai H.
j. Am. Chem. Soc. 2012,
134, 15849-15857.).Although people have carried out a large amount of research for this reason, the catalyst of ORR does not still reach the level of our expectation at present.Develop efficient, cheap ORR catalyst and remain a very large challenge.
In addition, research finds to mix Graphene class material by nitrogen, and for ORR, reaction has good castering action, but correlative study at present is only confined to the field of compound material that nitrogen is mixed Graphene and nano particle.
Summary of the invention
The object of the invention is to propose the preparation method that a kind of nitrogen of hyperoxia reducing property is mixed Graphene-niobium pentaoxide intercalation composite catalyst.
The present invention proposes the preparation method that a kind of nitrogen of hyperoxia reducing property is mixed Graphene-niobium pentaoxide intercalation composite catalyst, and concrete steps are as follows:
(1) niobium pentaoxide and potash are mixed according to the molar ratio of 3:1-3:1.5, be heated to 600-1000 ℃ and maintain 1 hour;
(2), by the product of step (1) gained, continue to be heated to 1050-1300 ℃ and maintain 1-10 hour;
(3) product of step (2) gained is fully washed with hot water; And at 100-500 ℃ dry 1-72 hour;
(4) product of step (3) gained is placed in to the salpeter solution of 10-68 wt%, stirs 1-7 days; Repeat 2-5 time;
(5) product of step (4) gained is filtered and fully washed with distilled water, afterwards 30-80 ℃ of dry 1-72 hour;
(6) after being mixed with mass ratio 1:0.2-1:5 with 4-vinylpridine, the product of step (5) gained is distributed in water;
(7) mixture of step (6) gained is at room temperature stirred to 1-7 days;
(8) product of step (7) gained is filtered, with distilled water washing, and vacuum drying 1-72 hour at room temperature;
(9) product of step (8) gained is heated under argon gas atmosphere to 700-900 ℃ and maintain 1-10 hour, obtains target product after cooling.
In the present invention, the niobium pentaoxide of step (1) and potash mol ratio 3:1.05-3:1.3.Preferably, the niobium pentaoxide of step (1) and potash mol ratio are 3:1.1.
In the present invention, the heating-up temperature of step (1) is 750-850 ℃; Heating-up temperature is 1100-1250 ℃, holds time as 4-6 hour.Preferably, the heating-up temperature of step (1) is 800 ℃; The heating-up temperature of step (2) is 1200 ℃, and holding time is 5 hours.
In the present invention, the baking temperature of step (3) is 120-300 ℃, and be 12-36 hour drying time.Preferably, the baking temperature of step (3) is 200 ℃, and be 24 hours drying time.
In the present invention, the concentration of nitric acid in step (4) is 20-60 wt%, stirs 2-5 days; Repeat 3-4 time.Preferably, the concentration of nitric acid in step (4) is 40 wt%, stirs 2 days; Repeat 3 times.
In the present invention, the baking temperature in step (5) is 40-60 ℃, and the time is 12-36 hour.Preferably, the baking temperature in step (5) is 50 ℃, and the time is 24 hours.
In the present invention, product and the 4-vinylpridine mass ratio of step (5) gained described in step (6) are 1:0.5-1:2.Preferably, product and the 4-vinylpridine mass ratio of step (5) gained in step (6) are 1:1.
In the present invention, in step (7), mixing time is 2-5 days.Preferably, the mixing time in step (7) is 3 days.
In the present invention, be 12-36 hour the drying time in step (8).Preferably, be 24 hours the drying time in step (8).
In the present invention, the heating-up temperature in step (9) is 750-850 ℃, holds time as 4-8 hour.Preferably, the heating-up temperature in step (9) is 800 ℃, and holding time is 6 hours.
The present invention, by the reaction condition of optimizing, can obtain nitrogen and mix Graphene-niobium pentaoxide intercalation composite catalyst (N-graphene-Nb
2o
5).This material has showed splendid catalytic effect in oxygen reduction reaction, has shown than the better stability of current representational Pt/C catalyst, higher methanol tolerance and suitable take-off potential.
Accompanying drawing explanation
Fig. 1 is 4000x SEM (SEM) photo that nitrogen is mixed Graphene-niobium pentaoxide intercalation composite catalyst;
Fig. 2 is 10000x SEM (SEM) photo that nitrogen is mixed Graphene-niobium pentaoxide intercalation composite catalyst;
Fig. 3 is the oxygen reduction reaction test result that nitrogen is mixed Graphene-niobium pentaoxide intercalation composite catalyst;
Fig. 4 is the electrochemical stability test result that nitrogen is mixed Graphene-niobium pentaoxide intercalation composite catalyst;
Fig. 5 is the electrochemistry methanol tolerance test result that nitrogen is mixed Graphene-niobium pentaoxide intercalation composite catalyst.
The specific embodiment
The following examples are to further illustrate of the present invention, rather than limit the scope of the invention.
Embodiment 1
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, can obtains target catalyst material after cooling.
The typical SEM photo that EXAMPLE l successfully makes target catalyst material as shown in Figure 1, 2.Its typical oxygen reduction reaction test result as shown in Figure 3.The typical test results that its methanol tolerance disturbs (be take Pt/C as contrast) as shown in Figure 4.Its stability test result (be take Pt/C as contrast) as shown in Figure 5.
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 300 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, can obtains target catalyst material after cooling.
Embodiment 3
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 3 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, can obtains target catalyst material after cooling.
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:2 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, can obtains target catalyst material after cooling.
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1150 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, can obtains target catalyst material after cooling.
Embodiment 6
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1, the mixture of gained is heated to 600 ℃ and maintain 1 hour, continue to be heated to 1050 ℃ and maintain 10 hours.The product hot wash obtaining, and be dried 72 hours at 100 ℃.The product obtaining is placed in to the salpeter solution of 10 wt%, stirs 7 days; Repeat 5 times.The product obtaining is filtered and wash with distilled water, 30 ℃ are dried 72 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 7 days after mixing with mass ratio 1:0.2 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 72 hours.The product obtaining is heated under argon atmospher to 700 ℃ and maintain 10 hours, can obtains target catalyst material after cooling.
Embodiment 7
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.05, the mixture of gained is heated to 850 ℃ and maintain 1 hour, continue to be heated to 1100 ℃ and maintain 6 hours.The product hot wash obtaining, and be dried 36 hours at 120 ℃.The product obtaining is placed in to the salpeter solution of 20 wt%, stirs 5 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 60 ℃ are dried 12 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 2 days after mixing with mass ratio 1:2 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 12 hours.The product obtaining is heated under argon atmospher to 750 ℃ and maintain 8 hours, can obtains target catalyst material after cooling.
Embodiment 8
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.3, the mixture of gained is heated to 750 ℃ and maintain 1 hour, continue to be heated to 1250 ℃ and maintain 4 hours.The product hot wash obtaining, and be dried 12 hours at 300 ℃.The product obtaining is placed in to the salpeter solution of 60 wt%, stirs 2 days; Repeat 2 times.The product obtaining is filtered and wash with distilled water, 40 ℃ are dried 36 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 1 day after mixing with mass ratio 1:5 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 1 hour.The product obtaining is heated under argon atmospher to 850 ℃ and maintain 4 hours, can obtains target catalyst material after cooling.
Embodiment 9
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.5, the mixture of gained is heated to 1000 ℃ and maintain 1 hour, continue to be heated to 1300 ℃ and maintain 1 hour.The product hot wash obtaining, and be dried 1 hour at 500 ℃.The product obtaining is placed in to the salpeter solution of 68wt%, stirs 1 day; Repeat 4 times.The product obtaining is filtered and wash with distilled water, 80 ℃ are dried 1 hour afterwards.The product obtaining is distributed in water and at room temperature stirs 5 days after mixing with mass ratio 1:0.5 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 36 hours.The product obtaining is heated under argon atmospher to 900 ℃ and maintain 1 hour, can obtains target catalyst material after cooling.
From above-described embodiment 1-9, in the condition and range of setting in the present invention, all can obtain target catalyst material.
Comparative example 1:
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 500 ℃ and maintain 1 hour, continue to be heated to 800 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, cannot obtains target material after cooling.From above-mentioned experiment, if the sintering temperature of niobium pentaoxide and potash is too low, cannot form corresponding intermediate product, can not get target catalyst material.
Comparative example 2:
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 2wt%, stirs 1 day; Repeat 2 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, cannot obtains target material after cooling.From above-mentioned experiment, if the concentration of nitric acid treatment is too low, cannot form corresponding intermediate product, can not get target catalyst material.
Comparative example 3:
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 200 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 800 ℃ and maintain 6 hours, cannot obtains target material after cooling.From above-mentioned experiment, if the product after nitric acid treatment is carried out to the dry of excessive temperature, can destroy the structure of corresponding intermediate product, can not get target catalyst material.
Comparative example 4:
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under argon atmospher to 500 ℃ and maintain 6 hours, cannot obtains target material after cooling.From above-mentioned experiment, if the sintering temperature under final step argon atmospher is too low, cannot there is effective conversion, can not get target catalyst material.
Comparative example 5:
Niobium pentaoxide and potash are mixed according to the molar ratio of 3:1.1, the mixture of gained is heated to 900 ℃ and maintain 1 hour, continue to be heated to 1200 ℃ and maintain 5 hours.The product hot wash obtaining, and be dried 24 hours at 200 ℃.The product obtaining is placed in to the salpeter solution of 40 wt%, stirs 2 days; Repeat 3 times.The product obtaining is filtered and wash with distilled water, 50 ℃ are dried 24 hours afterwards.The product obtaining is distributed in water and at room temperature stirs 3 days after mixing with mass ratio 1:1 with 4-vinylpridine.By the product that obtains filter, with distilled water washing, and at room temperature vacuum drying 24 hours.The product obtaining is heated under air atmosphere to 800 ℃ and maintain 6 hours, cannot obtains target material after cooling.From above-mentioned experiment, if final step atmosphere is selected air, cannot there is effective conversion, can not get target catalyst material.
Claims (10)
1. the nitrogen of hyperoxia reducing property is mixed a preparation method for Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that concrete steps are as follows:
(1) by niobium pentaoxide and potash according to the mixed in molar ratio of 3:1-3:1.5, be heated to 600-1000 ℃ and maintain 50-70 minute;
(2), by the product of step (1) gained, continue to be heated to 1050-1300 ℃ and maintain 1-10 hour;
(3) product of step (2) gained is fully washed with hot water; And at 100-500 ℃ dry 1-72 hour;
(4) product of step (3) gained is placed in to the salpeter solution of 10-68 wt%, stirs 1-7 days; Repeat 2-5 time;
(5) product of step (4) gained is filtered and fully washed with distilled water, afterwards 30-80 ℃ of dry 1-72 hour;
(6) after being mixed with mass ratio 1:0.2-1:5 with 4-vinylpridine, the product of step (5) gained is distributed in water;
(7) mixture of step (6) gained is at room temperature stirred to 1-7 days;
(8) product of step (7) gained is filtered, with distilled water washing, and vacuum drying 1-72 hour at room temperature;
(9) product of step (8) gained is heated under argon gas atmosphere to 700-900 ℃ and maintain 1-10 hour, obtains target product after cooling.
2. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that step (1) described niobium pentaoxide and potash mol ratio are 3:1.05-3:1.3.
3. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described heating-up temperature of step (1) is 750-850 ℃; The described heating-up temperature of step (2) is 1100-1250 ℃, holds time as 4-6 hour.
4. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described baking temperature of step (3) is 120-300 ℃, and be 12-36 hour drying time.
5. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described concentration of nitric acid of step (4) is 20-60 wt%, stirs 2-5 days; Repeat 3-4 time.
6. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described baking temperature of step (5) is 40-60 ℃, and the time is 12-36 hour.
7. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that product and the 4-vinylpridine mass ratio of the described gained of step (5) that step (6) is described is 1:0.5-1:2.
8. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described mixing time of step (7) is 2-5 days.
9. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that step (8) described drying time is 12-36 hour.
10. the nitrogen of a kind of hyperoxia reducing property according to claim 1 is mixed the preparation method of Graphene-niobium pentaoxide intercalation composite catalyst, it is characterized in that the described heating-up temperature of step (9) is 750-850 ℃, holds time as 4-8 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837426A (en) * | 2016-04-22 | 2016-08-10 | 上海交通大学 | Method for producing lactic acid by carrying out hydrothermal conversion on carbohydrate biomass |
| CN109499595A (en) * | 2018-11-16 | 2019-03-22 | 中国林业科学研究院林产化学工业研究所 | A kind of oxygen reduction reaction (ORR) catalyst GPNCS and preparation method thereof |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
| CN113717589A (en) * | 2021-09-09 | 2021-11-30 | 徐州特之达包装科技有限公司 | Waterproof self-cleaning fiber coating and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012128287A1 (en) * | 2011-03-24 | 2012-09-27 | 国立大学法人横浜国立大学 | Oxygen reduction catalyst and methods for preparing same |
| CN103007976A (en) * | 2012-12-11 | 2013-04-03 | 湖南科技大学 | Doped polyaniline directly-carbonized composite electrocatalyst, preparation method and application |
| CN103143319A (en) * | 2013-03-01 | 2013-06-12 | 暨南大学 | Graphene/clay composite material, and preparation method and application thereof |
| CN103254429A (en) * | 2013-05-21 | 2013-08-21 | 合肥工业大学 | Preparation method of polyaniline and molybdenum disulfide intercalated composite material |
| CN103274393A (en) * | 2013-05-24 | 2013-09-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing nitrogen-doped graphene and nitrogen-doped graphene |
-
2013
- 2013-11-27 CN CN201310606812.6A patent/CN103657698B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012128287A1 (en) * | 2011-03-24 | 2012-09-27 | 国立大学法人横浜国立大学 | Oxygen reduction catalyst and methods for preparing same |
| CN103007976A (en) * | 2012-12-11 | 2013-04-03 | 湖南科技大学 | Doped polyaniline directly-carbonized composite electrocatalyst, preparation method and application |
| CN103143319A (en) * | 2013-03-01 | 2013-06-12 | 暨南大学 | Graphene/clay composite material, and preparation method and application thereof |
| CN103254429A (en) * | 2013-05-21 | 2013-08-21 | 合肥工业大学 | Preparation method of polyaniline and molybdenum disulfide intercalated composite material |
| CN103274393A (en) * | 2013-05-24 | 2013-09-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing nitrogen-doped graphene and nitrogen-doped graphene |
Non-Patent Citations (1)
| Title |
|---|
| ZHIJIAN YANG ET AL.: "Layered niobic acid with self-exfoliatable nanosheets and adjustable acidity for catalytic hydration of ethylene oxide", 《JOURNAL OF CATALYSIS》, vol. 280, 6 May 2011 (2011-05-06) * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837426A (en) * | 2016-04-22 | 2016-08-10 | 上海交通大学 | Method for producing lactic acid by carrying out hydrothermal conversion on carbohydrate biomass |
| CN109499595A (en) * | 2018-11-16 | 2019-03-22 | 中国林业科学研究院林产化学工业研究所 | A kind of oxygen reduction reaction (ORR) catalyst GPNCS and preparation method thereof |
| CN109499595B (en) * | 2018-11-16 | 2021-10-08 | 中国林业科学研究院林产化学工业研究所 | Oxygen Reduction Reaction (ORR) catalyst GPNCS and preparation method thereof |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
| CN109980210B (en) * | 2019-04-19 | 2021-01-29 | 陕西科技大学 | Niobium pentoxide three-dimensional doped graphene composite material and preparation method and application thereof |
| CN113717589A (en) * | 2021-09-09 | 2021-11-30 | 徐州特之达包装科技有限公司 | Waterproof self-cleaning fiber coating and preparation method thereof |
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